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Volume 69 
Part 12 
Pages m635-m636  
December 2013  

Received 20 October 2013
Accepted 28 October 2013
Online 6 November 2013

Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](C-C) = 0.005 Å
R = 0.041
wR = 0.092
Data-to-parameter ratio = 15.4
Details
Open access

Di-[mu]-oxido-bis­({2,2'-[ethane-1,2-diylbis(nitrilo­methanylyl­idene)]diphen­olato}titanium(IV)) chloro­form disolvate

aDepartment of Chemistry, M.V. Lomonosov Moscow State University, Leninskie Gory 1/3, Moscow 119991, Russian Federation,bBelarussian State University, Phys. Chem. Problems Res. Inst., 14 Leningradskaya St, Minsk 220030, Republic of Belarus, and cInstitute of General and Inorganic Chemistry, Russian Academy of Sciences, Leninskii Prosp. 31, Moscow 119991, Russian Federation
Correspondence e-mail: churakov@igic.ras.ru.ru

In the title structure, [Ti2(C16H16N2O2)2O2]·2CHCl3, the Ti atom is coordinated in a distorted octa­hedral geometry by the O,N,N',O' donor set of the salalen ligand and by two [mu]2-oxide O atoms, which bridge two Ti(salalen) fragments into a centrosymmetric dimeric unit. In the central Ti2([mu]2-O)2 fragment, the metal-oxygen distances are significantly different [1.7962 (19) and 1.9292 (19) Å]. In the crystal, the chloro­form mol­ecule is anchored via an N-H...Cl and a bifurcated C-H...(O,O) hydrogen bond. Slipped [pi]-[pi] stacking [shortest C...C distance = 3.585 (4) Å] and C-H...[pi] inter­actions contribute to the coherence of the structure.

Related literature

For general background to the chemistry affording the tetra­dentate salalen ligand, see: Matsumoto et al. (2005[Matsumoto, K., Sawada, Y., Saito, B., Sakai, K. & Katsuki, T. (2005). Angew. Chem. Int. Ed. 44, 4935-4939.], 2007[Matsumoto, K., Saito, B. & Katsuki, T. (2007). Chem. Commun. pp. 3619-3627.]). For the crystal structure of a salalen complex, see: Taylor et al. (2006[Taylor, M. K., Reglinski, J., Berlouis, L. E. A. & Kennedy, A. R. (2006). Inorg. Chim. Acta, 359, 2455-2464.]). For the structure of the parent titanium salen compound, see: Tsuchimoto (2001[Tsuchimoto, M. (2001). Bull. Chem. Soc. Jpn, 74, 2101-2105.]). For our previous work on titanium(IV) complexes with polydentate N,O-ligands, see: Zaitsev et al. (2006[Zaitsev, K. V., Karlov, S. S., Selina, A. A., Oprunenko, Yu. F., Churakov, A. V., Neumüller, B., Howard, J. A. K. & Zaitseva, G. S. (2006). Eur. J. Inorg. Chem. pp. 1987-1999.], 2008[Zaitsev, K. V., Bermeshev, M. V., Samsonov, A. A., Oprunenko, J. F., Churakov, A. V., Howard, J. A. K., Karlov, S. S. & Zaitseva, G. S. (2008). New J. Chem. 32, 1415-1431.]).

[Scheme 1]

Experimental

Crystal data
  • [Ti2(C16H16N2O2)2O2]·2CHCl3

  • Mr = 903.15

  • Triclinic, [P \overline 1]

  • a = 10.237 (3) Å

  • b = 10.356 (3) Å

  • c = 10.936 (3) Å

  • [alpha] = 117.075 (4)°

  • [beta] = 93.113 (4)°

  • [gamma] = 110.463 (4)°

  • V = 935.0 (4) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 0.91 mm-1

  • T = 150 K

  • 0.08 × 0.06 × 0.01 mm

Data collection
  • Bruker SMART APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.931, Tmax = 0.991

  • 8213 measured reflections

  • 3668 independent reflections

  • 2761 reflections with I > 2[sigma](I)

  • Rint = 0.037

Refinement
  • R[F2 > 2[sigma](F2)] = 0.041

  • wR(F2) = 0.092

  • S = 1.03

  • 3668 reflections

  • 238 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.41 e Å-3

  • [Delta][rho]min = -0.43 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1 and Cg2 are the centroids of the C11-C16 and C21-C26 rings, respectively.

D-H...A D-H H...A D...A D-H...A
N2-H2...Cl3i 0.81 (3) 2.84 (3) 3.575 (3) 151 (3)
C1-H1...O2 1.00 2.55 3.506 (4) 160
C1-H1...O3 1.00 2.51 3.257 (4) 131
C17-H17...Cg2ii 0.95 2.81 3.754 (4) 174
C23-H23...Cg1iii 0.95 2.86 3.747 (4) 156
Symmetry codes: (i) -x+1, -y+1, -z; (ii) -x+1, -y+2, -z; (iii) x-1, y, z.

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: QK2062 ).


Acknowledgements

This work was partially supported by the RFBR (project 12-03-90020-Bel_a) and a grant from the President of the Russian Federation to support the research of young Russian scientists and doctors (MD-3634.2012.3).

References

Bruker (2008). APEX2, SADABS and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Matsumoto, K., Saito, B. & Katsuki, T. (2007). Chem. Commun. pp. 3619-3627.  [CrossRef]
Matsumoto, K., Sawada, Y., Saito, B., Sakai, K. & Katsuki, T. (2005). Angew. Chem. Int. Ed. 44, 4935-4939.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Taylor, M. K., Reglinski, J., Berlouis, L. E. A. & Kennedy, A. R. (2006). Inorg. Chim. Acta, 359, 2455-2464.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Tsuchimoto, M. (2001). Bull. Chem. Soc. Jpn, 74, 2101-2105.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Zaitsev, K. V., Bermeshev, M. V., Samsonov, A. A., Oprunenko, J. F., Churakov, A. V., Howard, J. A. K., Karlov, S. S. & Zaitseva, G. S. (2008). New J. Chem. 32, 1415-1431.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Zaitsev, K. V., Karlov, S. S., Selina, A. A., Oprunenko, Yu. F., Churakov, A. V., Neumüller, B., Howard, J. A. K. & Zaitseva, G. S. (2006). Eur. J. Inorg. Chem. pp. 1987-1999.  [Web of Science] [CSD] [CrossRef]


Acta Cryst (2013). E69, m635-m636   [ doi:10.1107/S1600536813029656 ]

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